CN1124879C - Preparation process of alumina adsorbant - Google Patents
Preparation process of alumina adsorbant Download PDFInfo
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- CN1124879C CN1124879C CN 00136212 CN00136212A CN1124879C CN 1124879 C CN1124879 C CN 1124879C CN 00136212 CN00136212 CN 00136212 CN 00136212 A CN00136212 A CN 00136212A CN 1124879 C CN1124879 C CN 1124879C
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Abstract
The present invention provides a method for preparing an adsorbing agent by utilizing activated alumina to support alkali (soil) metal compounds, which relates to the technical field of preparing catalysts and adsorbing agents. Aluminium hydroxide is used as raw material, and the raw material is dried and pulverized to a certain mesh number and then is rapidly dehydrated in high-temperature air streams to obtain initial powder of activated alumina. The initial powder is put into a disk type granulator, and water solution of alkali (soil) metal compounds is sprayed in. Finished products are obtained through rolling molding and calcination. The product has the advantages of high adsorption capacity, large pore volume, large specific surface area and high crushing resistant strength and can obviously improve catalytic activity.
Description
The present invention relates to catalyst, adsorbent manufacturing technology field, exactly prepare the method for adsorbent for a kind of activated alumina load alkali (soil) components of metal compounds.
The present invention's technology in the past, the manufacturing of activated alumina generally have acid-base neutralization method, rapid dehydration method, aluminium alcoholates method etc.The activated alumina that is used in adsorbing domain is generally by rapid dehydration method production, and promptly aluminium hydroxide makes the active oxidation aluminium powder of porous through the high temperature gas flow fast dewatering, makes finished product through moulding, calcining again, the invention belongs to the expansion of this technology.
The present invention is directed to the problem of commercially available activated alumina in some absorption and catalytic field existence, a kind of preparation method of the activated alumina that contains alkali (soil) metallic compound of novelty is provided, product by this method preparation has higher adsorption capacity, pore volume and specific area and crushing strength, can significantly improve catalytic activity.
The present invention realizes in the following manner: be raw material with aluminium hydroxide, drying, be crushed to certain order number, in high temperature gas flow through fast dewatering, make the former powder of activated alumina, former powder is placed in the dribbling balling machine, sprays into the aqueous solution of alkali (soil) metallic compound, the rolling moulding, through calcining, get finished product again.
The technical process of preparation is:
(1) the aluminium hydrate powder bake out temperature is at 100 ℃-140 ℃, and is crushed to below 300 orders.
(2) in the high temperature gas flow with 380 ℃-1000 ℃ of aluminium hydroxide fine powder addings,, make the active oxidation aluminium powder of porous through instantaneous fast dewatering.
(3) aqueous solution of preparation alkali or strong base-weak acid salt is made adhesive, and control pH value is in the 11-14 scope.
(4) the active oxidation aluminium powder is put into dribbling balling machine, spray into the adhesive of above-mentioned (3) preparation, the rolling moulding.
(5) will become the semi-finished product of type to handle 3-16 hour down at 30 ℃-120 ℃, the calcining furnace of packing into was calcined 1-4 hour down at 300 ℃-450 ℃, made product of the present invention.
Aluminium hydroxide can adopt β-gibbsite, α-gibbsite or boehmite in above-mentioned (1), preferably adopts β-gibbsite or α-gibbsite.
In above-mentioned (2), when thin aluminium hydrate powder dewatered in thermal current, the time of staying was 0.1-5 second, and dehydration temperaturre is preferably in 380 ℃-900 ℃ at 300 ℃-1000 ℃.
In above-mentioned (3), alkali (soil) metallic compound calcining back exists with the metal oxide form on aluminium oxide.Concentration range is between 0.5-15%, and pH value scope is preferably between the 12-13.7.This aqueous solution can be one or more mixture.
In the above-mentioned technical process (4), the adding of when the rolling moulding, spraying of the solution of preparation.
In the above-mentioned technical process (5), temperature retention time is more than 5 hours.
In the above-mentioned technical process (5), temperature retention time is more than 10 hours.
In the above-mentioned technical process (5), the temperature of calcining is 300-550 ℃.
In above-mentioned (5), the time of calcining generally between 0.5-4 hour, is preferably in 40 minutes to 2 hours.The temperature of calcining is preferably between 380 ℃-420 ℃.
The catalyst of the present invention's preparation has following performance:
Compressive resistance: 〉=60N/cm; Specific area: 〉=280m
2/ g;
Bulk specific weight: 0.6-0.9g/ml; Pore volume: 〉=0.40ml/g;
Burning decrement (1000 ℃, 2h): 3-9%, w/w;
Characteristic of the present invention is:
1. prepare certain density alkali (soil) metal compound solution, control pH value is between 12.7-13.5.
2. Pei Zhi the aqueous solution can be the solution that simple aqueous slkali, strong base weak acid salting liquid or aqueous slkali neutralizes with acid, it also can be the mixture of several solns, as sodium hydroxide solution, potassium hydroxide solution, magnesium hydroxide solution, aqua calcis, lithium hydroxide solution, sodium carbonate liquor, sodium acetate solution, sodium formate solution, or the solution that neutralizes with acid as nitric acid, carbon dioxide, organic acid of NaOH, potassium hydroxide solution.
3. alkali (soil) metallic compound is with aqueous solution form, and spraying adds during the rolling moulding in dribbling balling machine.
4. to have intensity good for the activated alumina of the present invention preparation, and pore volume, specific area increase, and simultaneously, adsorption capacity is significantly increased.
5. the product of the present invention's preparation is specially adapted to gas or the adsorbing and removing of other acidic materials and the regenerated catalysts of anthraquinone preparation hydrogen peroxide industry degradation product such as hydrogen chloride in the petro chemical industry, carbon dioxide, hydrogen sulfide.
That activated alumina production technology of the present invention has is simple to operate, product strength good, pore volume and specific area are big, characteristics such as result of use is good.
Embodiment 1
Do raw material with commercially available α-gibbsite, 120 ℃ of oven dry down, be crushed to 325 orders, through 450-780 ℃ of fast dewatering, get amorphous active oxidation aluminium powder, put into dribbling balling machine, spray into water and pH value respectively 12.0,13.0,13.5 sodium hydroxide solution, rolling is formed into φ 1.5-2.9mm.Semi-finished product are 40 ℃ of following healths 11 hours, under 400 ℃, calcine the finished product activated alumina.
The product that makes has following result after tested:
Lot number | Specific area (m 2/g) | Pore volume (ml/g) | Compression strength (N/) | Bulk specific weight (g/ml) |
Pure water | 292 | 0.39 | 47 | 0.77 |
pH12.7 | 298 | 0.40 | 55 | 0.80 |
pH13.0 | 318 | 0.41 | 57 | 0.82 |
pH13.5 | 332 | 0.43 | 66 | 0.84 |
Embodiment 2
Do raw material with commercially available α-gibbsite, 120 ℃ of oven dry down, be crushed to 325 orders, through 450-780 ℃ of fast dewatering, amorphous active oxidation aluminium powder, put into dribbling balling machine, spray into water and 5%, 12% sodium hydroxide solution respectively, wherein 13.5, roll is formed into φ 3.0-5.0mm to sodium hydroxide solution with rare nitre acid for adjusting pH value.Semi-finished product are 40 ℃ of following healths 11 hours, under 400 ℃, calcine the finished product activated alumina.
The product that makes has following result after tested:
Lot number | Specific area (m 2/g) | Pore volume (m/g) | Compression strength (N/) | Bulk specific weight (g/ml) | Na 2O content (w/w, %) |
Pure water | 287 | 0.38 | 147 | 0.71 | 0.41 |
5% | 311 | 0.41 | 183 | 0.78 | 1.62 |
12% | 290 | 0.43 | 195 | 0.81 | 3.77 |
Claims (9)
1. preparation method who contains the activated alumina adsorbents of alkaline earth, with aluminium hydroxide is raw material, drying, pulverizing are dewatered in thermal current, make the former powder of activated alumina, former powder is placed in the dribbling balling machine, spray into the aqueous solution of alkaline earth metal compound, the rolling moulding is again through calcining, get finished product, it is characterized in that:
(1) the aluminium hydrate powder bake out temperature is at 100 ℃-140 ℃, and is crushed to 300 orders;
(2) in the high temperature gas flow with 380 ℃-1000 ℃ of aluminium hydrate powder addings,, make the active oxidation aluminium powder of porous through dehydration;
(3) aqueous solution of preparation alkali or strong base-weak acid salt is made adhesive, and its pH value is 11-14;
(4) the active oxidation aluminium powder is put into dribbling balling machine, spray into the solution of (3), the rolling moulding;
(5) be incubated 3-16 hour down at 30 ℃-120 ℃, the calcining furnace of packing into was calcined 0.5-4 hour down at 300 ℃-450 ℃, made product of the present invention.
2. according to the preparation method of claim 1, it is further characterized in that: aluminium hydroxide β-gibbsite, α-gibbsite or boehmite.
3. according to the preparation method of claim 1, it is further characterized in that: the aqueous solution of preparation is the solution that simple aqueous slkali, strong base weak acid salting liquid or aqueous slkali neutralizes with acid, or the mixture of several solns.
4. according to the preparation method of claim 1, it is further characterized in that: the pH value of the solution of preparation is 12-13.7.
5. according to the preparation method of claim 1, it is further characterized in that: the adding of spraying when the rolling moulding of the solution of preparation.
6. according to the preparation method of claim 1, it is further characterized in that: temperature retention time is more than 5 hours.
7. according to the preparation method of claim 6, it is further characterized in that: temperature retention time is more than 10 hours.
8. according to the preparation method of claim 1, it is further characterized in that: the temperature of calcining is 300-550 ℃.
9. according to the preparation method of claim 8, it is further characterized in that: the temperature of calcining is 380-420 ℃.
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CN 00136212 CN1124879C (en) | 2000-12-25 | 2000-12-25 | Preparation process of alumina adsorbant |
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CN 00136212 CN1124879C (en) | 2000-12-25 | 2000-12-25 | Preparation process of alumina adsorbant |
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CN1307929A CN1307929A (en) | 2001-08-15 |
CN1124879C true CN1124879C (en) | 2003-10-22 |
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